Apparatus for producing tetrahalogenated hydrocarbons



w. H. RODEBUSH.

APPARATUS FOR PRODUCING TETBAHALOGENATED HYDROCARBONS.

APPLICATION 'FILED AUGZS, ms.

1,402,318, Patented Jan. 3, 1922,

UNITED STATES PATENT OFFICE.

fwon'ra H. nonnnnsn', or summons, nAnYLANn, assrenon To U. s. mnus'mm monor. 00., A oonronarron or wns'r vmemn.

AIPABAITUS IQR PRODUCING- TETRAEALOGENATED EYDROOARBONS.

To all whom it may concern:

Be it known that I, WORTH a citizen of the United States, residing at Baltimore, in the State of Maryland, have 1 tetrachloridev or the corresponding compounds of acetylene with other halogens may be advantageously made. Another object of my invention is to provide an apparatus of this character in which a high yield is obtained. Still another object is to provide anlapparatus of this character which is conducted so as to avoid the esoape'of the reagents and the products desired formed.

; urther objects of my invention will appear from the detailed description thereof contained hereinafter.

While my invention is capable of embodiment in many different forms, for the purpose of illustration I have shown only one form of apparatus in the accompanying drawing, in which: e

The figure is a diagrammatic representation of an apparatus made in accordance with my invention.

In the drawing, I have shown a container 1 which is preferably made of some opaque material, that will not be acted upon by the substances present therein during thetreatment. The container 1 is provided with a valved inlet opening 2 preferably inits top, as shown, and suitable for the liquid materials to be introduced into the container 1, and which is provided also for the purpose of permitting the insertion of a thermometer to determine the temperatures during'the treatment. As above indicated, the apparatus may be utilized for producing acetylene tetrachloride, acetylene tetrabromide, or acetylene tetraiodide, but I shall describe it particularly as'applied to the production of Specification of Letters Patent.

H; RonEBUsn,

Patented Jan. 3, 1922.

' Application filed August 25, 1919. Serial No. 319,731.

acetylene tetrachloride. For this purpose, I introduce into the container 1 through-the valved inlet opening2 a quantity of ethylene dichloride. After the valved inlet opening 2 has been closed, gaseous chlorine is intro-' duced by means ofan annular perforated pipe 3 located near the bottom of the container 1,so as to thereby agitate the liquid,

and cause the chlorine-to become dissolved therein. The agitation of the liquid is augmented by the operation of mechanical means such as a propeller 4 carried by a shaft 5 in the container 1, and driven by bevel gears 6 and 7 from a driving shaft 8 carrying a pulley 9, which is driven from any suitable source of power.. The rotation of the propeller 4 produces a downward current of the materials in the container 1, tending to cause. the same to pass out through an opa ue tube 10, thence into a glass tube 11, an from this point by means of an opaque tube 12 back into the container 1. The circulation of the liquid in this manner is insured, however, by the presence of a propeller 12 in the tube" 10. In

this way, a continual circulation of the materials is obtained through the glass tube 11; In the interior of the tube 11 there is also shown a mercury vapor light 12 to provide actinic light when the light from the sun is insufficient. There is a considerable rise in temperature due to the combinaso as to form acetylene trichloride and acetylene' tetrachloride. The light admitted to the liquid through the transparent tube 11,

and the heat developed, both facilitate the union of the chlorine with-the ethylene dichloride, and in this way, the production of the acetylene tetrachloride is very much ae- 'celerated. During the treatment, there is an tion of chlorine with the ethylene dichloride,

water 15 and 16. The-reflux condenser will condense any of the ethylene dichloride,

acetylene trichloride and acetglene tetrachloride which may be vaporize during the treatment. Thetreatment is carried out in this way for from 2 to 3 hours, the liquid level being preferably maintained at about the point indicated in the drawing, and above the transparent chamber, and when the boiling point of the liquid has reached a temperature of ap roximately 104 (3.,

the action is stoppe and the liquid is' drawn off by means 'of a valved outlet pipe 17 located at the bottom of the container. This liquid will comprise a mixture of acetylene trichloride and acetylene tetrachloride with a little ethylene-dichloride, and these liquids may then be readily separated by fractional distillation.

It will be understood that instead of carrying out my invention in such a manner as to produce acetylene tetrachloride, ethylene dibromide may be treated by the injection of bromine in the form of a liquid or vapor stood that other temperatures may be employed according to the circumstances of the particular case and the character of the halogen. ingly be varied considerably from the temperature named, and no particular temperature is deemed essential, it being within the.

skill of those versed in the art to employ the proper temperature at which the action is to be stopped. L

I claim:

'1. A chlorinating apparatuscomprising a tank-having an inlet and outlet and a vertical reaction chamber connected thereto near its top and bottom, a source of light in the reaction chamber, an agitator at the bottom of the reaction chamber tojorce liquid up into it, and means for injecting chlorine into -the ta 2. A chlorinating apparatus comprising a tank having an inlet and outlet and a vertical reaction chamber connected thereto near its top and bottom, an agitator the tank operating to circulate liquid from the bottom of the tank up into the reaction chamber, a source of'light in the latter, an agitator at the bottom of the reaction chamber to force liquid thereinto, and means for injecting chlorine into the tank.

3. An apparatus for halogenating, 'com prising a main container provided with an inlet in'its u per portion and with an additional inlet or a halogen in its lower porv current therein,

The temperatures may accord-v tion, mechanical means for the agitation of the consequent mixture to produce a downward current therein, and a transparent re action chamber connected therewith by a plurality of tubes below the level of the iquid in saidmain container, whereby the mixture may be continuously circulated through the main chamber and the reaction tube, without danger of an excess of the halogen in the reaction chamber.

4. An apparatus for halogenating, comprising a mam container provided with an inlet in its u per portion and with an additional inletor a halogen in its lower portion, mechanical means for the agitation of the consequent mixture to produce a desired a transparent reaction chamber connected therewith by' a plurality of tubes below the level of the liquid in said main container and a mercury vapor light within said reaction tube, whereby the mixture. may be continuously circulated-through the main chamber andthe reaction tube, without danger of an excess of the halogen in the reaction chamber.

5. An apparatus for halogenating, comprising a main container provided with an inlet in its upper portion and with an inlet for a halogen in its lower portion, mechanical means for the agitation of the consequent mixture to produce a downward current therein, a transparent reactionchamber connected therewith by a plurality of tubes be low the level of the liquid in said'main container, and a reflux condenser connected to thetop of said main container, whereby the mixture may be continuously circulated through said main container and said reaction tube, without danger of an excess of the halogen in the reaction. chamber,j without loss of valued products.

6. An apparatus for halog'enatingfcomprising a main container provided with an inlet in its upper portion and with an inlet;

for a halogen in its lower portion, mechanical means for the agitation act the consequent mixture to produce a downward current therein, a transparent reaction tube below the level of the liquid in said main container, a source of light within said reconnected therewith by a plurality of tubes enation is carried to the desired degree of completion.

7. A chlorinating apparatus comprising a tion chamber connectedthereto near its top and bottom, a source of light in the reaction chamber, an agitator positioned to circulate tank having an inlet and outlet and a reacliquid from the tank through the reaction tioned to circulate liquid from the tank chamber, and means for injecting chlorine through the reaction chamber, and means 7 into the tank. I for injecting chlorine into the tank. 10 8. A chlorinating apparatus comprising a In testimony that I claim the foregoing, 5 tank having an inlet and outlet and a trans- I have hereunto set my hand this 31 day of parent reaction chamber connected thereto July, 1919. near its top and bottom, an agitator posi- WORTH H. RODEBUSH: 

